Preparation method of lithium manganese base-enriched ternary composite anode material

A composite positive electrode material, lithium-rich manganese-based ternary technology, applied in the preparation of lithium-rich manganese-based ternary composite materials, the field of preparation of lithium-rich manganese-based ternary composite positive electrode materials, can solve the problem of large particle size and wide particle size distribution , the first irreversible capacity of particle agglomeration and other issues, to achieve the effect of uniform particle size distribution, high energy density, and reduction of the first irreversible capacity

Inactive Publication Date: 2012-09-05
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the defects of large particle size, wide particle size distribution, particle agglomeration and large first irreversible capacity in the lithium-rich manganese-based ternary composite positive electrode material of lithium-ion secondary batteries in the prior art, the purpose of the present invention is to provide a rich A method for preparing a lithium-manganese-based ternary composite positive electrode material. The lithium-rich manganese-based ternary composite material prepared by the method is used as a positive electrode material for a lithium-ion secondary battery, and has small particle size, uniform particle size distribution, high activity, It can reduce the irreversible capacity for the first time and improve the cycle performance of the lithium-ion secondary battery using the material as the positive electrode material, etc.

Method used

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  • Preparation method of lithium manganese base-enriched ternary composite anode material
  • Preparation method of lithium manganese base-enriched ternary composite anode material
  • Preparation method of lithium manganese base-enriched ternary composite anode material

Examples

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Embodiment 1

[0042] (1) Dissolve 0.005 mol of nickel acetate, 0.005 mol of cobalt acetate and 0.02 mol of manganese acetate in 100ml of deionized water, and stir magnetically at 30°C for 4 hours to form a homogeneous mixed solution, in which Ni 2+ :Co 2+ :Mn 2+ The molar ratio of the substances is 1:1:4.

[0043] (2) Dissolve lithium hydroxide in deionized water and stir to dissolve to obtain 60ml of clear lithium hydroxide solution, in which the concentration of lithium hydroxide is 1.25mol / L; add the mixed solution dropwise to lithium hydroxide solution at a rate of 3ml / min The reaction solution was mixed with ammonia water to adjust the pH value of the reaction solution to 11.0, and the reaction solution was placed in a 50°C water bath and stirred at a speed of 120rmp for 3 hours, then aged for 4 hours, and the precipitate was obtained by suction filtration, and washed with distilled water for 3 hours. put the cleaned precipitate into the cold trap, and cool down to -90°C together wit...

Embodiment 2

[0052] (1) Dissolve 0.005mol of nickel acetate, 0.005mol of cobalt acetate and 0.02mol of manganese acetate in 100ml of deionized water, and stir magnetically at 35°C for 2 hours to form a homogeneous mixed solution, in which Ni 2+ :Co 2+ :Mn 2+ The molar ratio of the substances is 1:1:4.

[0053] (2) Dissolve 0.075mol of lithium hydroxide in deionized water and stir to obtain 60ml of clear lithium hydroxide solution, in which the concentration of lithium hydroxide is 1.25mol / L; add the mixed solution dropwise at a rate of 5ml / min. Mix the reaction solution with lithium solution, adjust the pH of the reaction solution to 8.0 with acetic acid, place the reaction solution in a water bath at 35°C at a speed of 100rmp and stir for 6 hours, then age it for 10 hours, filter it with suction to obtain the precipitate, and wash it with distilled water 3 times, and then washed 2 times with anhydrous ethanol to obtain the washed precipitate; first lower the temperature of the cold trap...

Embodiment 3

[0062] (1) Dissolve 0.005mol of nickel acetate, 0.005mol of cobalt acetate and 0.02mol of manganese acetate in 100ml of deionized water, and stir magnetically at 30°C for 12h to form a homogeneous mixed solution, in which Ni 2+ :Co 2+ :Mn 2+ The molar ratio of the substances is 1:1:4.

[0063] (2) Dissolve 2.9372g of lithium hydroxide in deionized water and stir to obtain 100ml of clear lithium hydroxide solution, in which, OH 1- The ratio of the substance to the metal ion is 1.2.1:1; the mixed solution and the lithium hydroxide solution are simultaneously added dropwise to a 60°C beaker at a rate of 10ml / min and mixed to obtain a reaction solution, and a constant temperature magnetic stirrer is used to continuously Stir the reaction solution, adjust the pH value of the reaction solution with acetic acid to be 8.5, stir the reaction at a speed of 500rmp for 3h, then age for 4h, obtain the precipitate by suction filtration, wash and wash 3 times with distilled water, and obta...

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Abstract

The invention relates to a preparation method of lithium manganese base-enriched ternary composite anode material, belonging to the field of green energy resource material. The method comprises the following steps of: stirring to make the mixture dissolve so as to obtain mixed solution; putting precipitator in the water to dissolve in a stirring way, so that precipitator solution can be obtained; mixing the mixed solution with the precipitator solution to obtain reaction liquid, adjusting the pH value of the reaction liquid into 7.0-12.0, stirring for reaction, aging, filtering to obtain precipitate, and washing the precipitate by detergent; cooling the washed precipitate into the temperature which is less than or equal to -10 DEG C, and freezing for the time which is more than or equal to 1h, and drying under the vacuum degree which is less than or equal to 10.0Pa, so that a precursor can be obtained; and mixing the precursor with the lithium salt to carry out thermal treatment, so that the lithium manganese base-enriched ternary composite anode material can be obtained. The material prepared by the method is small in granularity, even in particle size distribution, and high in activity, so that the first irreversible capacity can be reduced, and the cycle performance of the lithium ion secondary battery taking the material as the anode material can be improved.

Description

technical field [0001] The invention relates to a preparation method of a lithium-rich manganese-based ternary composite positive electrode material, specifically, the invention relates to a preparation method of a lithium-rich manganese-based ternary composite material used as a lithium-ion secondary battery positive electrode material, belonging to The field of green energy materials. Background technique [0002] As a new generation of rechargeable high-energy batteries, lithium-ion secondary batteries have many advantages such as high working voltage, high energy density, good safety performance, long cycle life and low self-discharge. After the successful commercialization of the secondary battery, it has been widely used in many portable electronic devices such as mobile phones, notebook computers and instruments. Application prospects. [0003] The cathode material of a lithium-ion secondary battery is one of the main factors affecting its cost and performance. The...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/10
Inventor 吴锋陈实仲云霞白莹吴川包丽颖吴伯荣
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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